CN109894472A - A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate - Google Patents
A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate Download PDFInfo
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Abstract
The present invention provides a kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate, dress powder is carried out according to the required suitable mold of molybdenum plate blank selection of dimension first, then the mold for filling powder is subjected to die mould and slab is made, the slab after die mould is sintered again, the rolling of aximal deformation value is carried out to sintered slab by the method for tandem rolling, improve the binding force between its interior tissue, pass through the available isotropic fiber fines tissue of tandem rolling, and vertically and horizontally organize interlaced overlap joint, tissue is more uniform, can effectively avoid it is each to discontinuity when the defect that generates, advantageous condition is provided for subsequent spinning, the present invention uses isostatic cool pressing, the tandem rolling method of sintering and aximal deformation value processes molybdenum raw material slab, it is set to meet the spinning requirement of big L/D ratio molybdenum crucible, life to big L/D ratio molybdenum crucible Production has great importance.
Description
Technical field
The invention belongs to molybdenum crucible processing technique fields, and in particular to a kind of big L/D ratio molybdenum crucible spinning molybdenum plate rolls
Method processed.
Background technique
Sapphire crystal (α-Al2O3) it is a kind of high temperature resistant, wear-resistant, anticorrosive and wide transmission region high-quality smooth function
Material or most popular oxide substrate (being mainly used as semiconductor substrate and large scale integrated circuit substrate) material it
One, it can be used for the fields such as microelectronics-photoelectron technology, military affairs, aerospace, communication, medicine, have broad application prospects.
Currently, sapphire single-crystal can be made there are many method, such as kyropoulos, Chai Shi crystal pulling method, EFG technique, heat exchange
The methods of method, temperature gradient method, Bridgman-Stockbarger method, cold core float die.In these methods, heat-exchanging method growth is blue precious
Stone monocrystalline needs to use the molybdenum crucible of the big L/D ratio of high-quality.
Molybdenum is a kind of refractory metal, and fusing point is 2620 DEG C, have extremely strong Binding Forces Between Atoms make it in room temperature and
High temperature strength is all very high；Molybdenum has the coefficient of expansion small, and conductivity is big, the excellent physical property such as good heat conductivity.These are excellent
Different performance makes molybdenum and its alloy be widely used in fields such as metallurgy, glass, ceramics, war industry equipment, high-temperature machineries.Molybdenum
The one kind of crucible as molybdenum materials, is widely used in during rare earth metal metallurgy, glass melting etc..Currently, the system of molybdenum crucible
Make method mainly include the following types: plasma spraying method, casting method, pressing, welding, sintering process etc..But plasma spray
Coating production especially wastes raw material and expensive；Casting method preparation process is complicated, needs to make a large amount of molds, and the fusing point of molybdenum
Height, fusing need to consume a large amount of electric energy；Pressing crucible biggish for wall thickness has good effect, but for large size, thin walled
Crucible technique realize difficulty it is larger；The crucible of welding welding easily cracks in commissure in use, reduces crucible
Service life；It is sintered the presence of molybdenum crucible hole during the sintering process, the strength reduction of molybdenum crucible can be made, influence making for molybdenum crucible
With.Spinning processing method is suitble to the processing to big L/D ratio thin-walled pressure vessel, but because this material of molybdenum belongs to refractory metal, relatively
It is larger in common metal spinning difficulty, and the molybdenum crucible spinning difficulty of big L/D ratio is bigger, common molybdenum crucible spinning molybdenum plate
Fibr tissue is thicker, and such tissue ductility is poor, is easy to produce crackle during spinning and causes scrap of the product.
Accordingly, it is desirable to provide a kind of for a kind of insufficient big L/D ratio molybdenum crucible spinning molybdenum plate of the above-mentioned prior art
Milling method.
Summary of the invention
The purpose of the present invention is to provide a kind of milling methods of big L/D ratio molybdenum crucible spinning molybdenum plate at least to solve
Big L/D ratio molybdenum crucible spinning molybdenum plate poor ductility at present, the problems such as being unfavorable for rotary pressure deformation.
To achieve the goals above, the invention provides the following technical scheme:
A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate, it is preferable that the milling method includes the following steps:
S1 feeds intake, and according to required molybdenum plate blank size, chooses the mold of suitable dimension, carries out dress powder；
S2, die mould carry out die mould processing to the mold for filling powder in step S1, the slab of suitable thickness are made；
S3, sintering are sintered the slab obtained of pressure in step S2；
S4, rolling, rolls sintered slab in step S3, obtains rolled parts；
S5, surface treatment, is surface-treated rolled parts obtained in step S4, and the surface for removing the rolled parts lacks
It falls into, obtains molybdenum plate rolled parts finished product.
A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as described above, it is preferable that in the step S2, adopt
Die mould is carried out to the mold for filling powder in step S1 with the forming method of equal static pressure.
A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as described above, it is preferable that in the step S2, adopt
Die mould is carried out to the slab chosen in step S1 with the forming method of isostatic cool pressing, the pressure that die mould uses for 200-220MPa,
Pressure maintaining 10-30 minutes.
A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as described above, it is preferable that further include shaping, to step
Slab obtained carries out shaping according to the shrinkage ratio in sintering process in rapid S2, to guarantee to obtain after sintering required size, smooth
Intact slab.
A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as described above, it is preferable that, will in the step S3
Slab after shaping, which is placed in sintering furnace, to be sintered, and maximum sintering temperature is 2000-2200 DEG C, keeps the temperature 3-5 hours.
A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as described above, it is preferable that the sintering furnace uses
Intermediate frequency furnace.
A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as described above, it is preferable that the step S4 is specific
Operating method are as follows: tandem rolling is carried out to slab sintered in the step S3 first, obtains rolled parts；Then it will obtain
Rolled parts carries out final annealing process；Rolled parts after finally extracting final annealing process carries out Mechanics Performance Testing, and test is moved back
The fracture elongation of rolled parts after fire.
A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as described above, it is preferable that the tandem rolling
Cheng Zhong, carries out split rolling method to slab sintered in step S3 first, and cogging temperature is controlled at 1150-1350 DEG C, using every
Passage melts down the mode of cooling rolling, cools down 30-100 DEG C per pass, and final rolling temperature is not less than 700 DEG C, in the operation of rolling
Middle to use horizontal and vertical alternate tandem rolling mode, tandem rolling obtains rolled parts；
Preferably, drafts during the rolling process per pass is 30%-40%；
More preferably, the total deformation of slab is controlled between 90%-98%.
A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as described above, it is preferable that the tool of the step S5
Gymnastics as: cleaning polishing is carried out to the surface of rolled parts obtained in step S4, removes the oxide skin on the rolled parts surface,
Polish off pit, the crackle local defect on the rolled parts surface.
A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as described above, it is preferable that the tandem rolling
Intert stress relief annealing process, 700-850 DEG C of the temperature of the stress relief annealing in journey；The annealing temperature of the final annealing process
Degree is 850-920 DEG C.
Compared with the immediate prior art, technical solution provided by the invention has following excellent effect:
The present invention provides a kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate, is carried out by isostatic cool pressing technology
Die mould obtains slab, obtains highdensity slab, is sintered by formulating sintering process to the slab after die mould, to improve it
Total quality；The rolling for carrying out aximal deformation value to sintered slab by the method for tandem rolling, makes between its interior tissue
Binding force improve, by the available isotropic fiber fines tissue of tandem rolling, and vertically and horizontally organize interlaced
Overlap joint, tissue more uniformly, can effectively avoid it is each to discontinuity when the defect that generates, provided for subsequent spinning advantageous
Condition, the present invention process molybdenum raw material slab using the tandem rolling method of isostatic cool pressing, sintering and aximal deformation value, make it
The spinning requirement for meeting big L/D ratio molybdenum crucible, has great importance to the production of big L/D ratio molybdenum crucible.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.
Wherein:
Fig. 1 is the preparation technology flow chart of the big L/D ratio molybdenum crucible spinning molybdenum plate of the embodiment of the present invention；
Fig. 2 is the big L/D ratio molybdenum crucible structural representation of the embodiment of the present invention；
Fig. 3 is the metallurgical tissue picture of the molybdenum plate of common process rolling；
Fig. 4 is the metallurgical tissue picture that the milling method of the embodiment of the present invention obtains.
Specific embodiment
The present invention will be described in detail below with reference to the accompanying drawings and embodiments.It should be noted that in the feelings not conflicted
Under condition, the features in the embodiments and the embodiments of the present application be can be combined with each other.
In the description of the present invention, term " longitudinal direction ", " transverse direction ", "upper", "lower", "front", "rear", "left", "right", " perpendicular
Directly ", the orientation or positional relationship of the instructions such as "horizontal", "top", "bottom" is to be based on the orientation or positional relationship shown in the drawings, and is only
For ease of description the present invention rather than require the present invention that must be constructed and operated in a specific orientation, therefore should not be understood as pair
Limitation of the invention.Term used in the present invention " connected ", " connection " shall be understood in a broad sense, for example, it may be fixedly connected,
It may be a detachable connection；It can be directly connected, can also be indirectly connected by intermediate member, for the common of this field
For technical staff, the concrete meaning of above-mentioned term can be understood as the case may be.
According to a particular embodiment of the invention, as depicted in figs. 1 and 2, the present invention provides a kind of big L/D ratio molybdenum crucible rotation
The pressure milling method of molybdenum plate, the milling method include the following steps:
S1 feeds intake, and according to required molybdenum plate blank size, chooses the gum cover mould of suitable dimension, carries out dress powder.
S2, die mould carry out die mould to the mold for filling powder in step S1 using the forming method of isostatic cool pressing；Die mould is adopted
Pressure is 200-220MPa (such as 202MPa, 205MPa, 208MPa, 212MPa, 215MPa, 218MPa), pressure maintaining 10-
30min (such as 12min, 15min, 18min, 23min, 28min).For the ease of subsequent rolling, in an embodiment of the present invention,
After die mould processing, shaping is carried out according to the shrinkage ratio in sintering process to the slab after die mould, to guarantee sintered slab
It is smooth intact, it is ready work for subsequent rolling, after sintering because of slab, intensity will greatly enhance, therefore selection is being pressed
Shaping is carried out after type, it is easy to process, save processing cost.
S3, sintering, is sintered the slab after step S2 medium-pressure type；Slab after shaping is placed in intermediate frequency furnace and is carried out
Sintering, maximum sintering temperature are 2000-2200 DEG C of (such as 2030 DEG C, 2060 DEG C, 2090 DEG C, 2120 DEG C, 2150 DEG C, 2180
DEG C), keep the temperature 3-5 hours (such as 3.2 hours, 3.5 hours, 3.8 hours, 4.0 hours, 4.2 hours, 4.5 hours, 4.8 hours).
Preferably, it is described sintering include: by the molybdenum plate blank after shaping be heated to 600-800 DEG C (such as 630 DEG C, 660 DEG C,
690 DEG C, 720 DEG C, 750 DEG C, 780 DEG C), keep the temperature 1-3 hours (such as 1.2 hours, 1.5 hours, 1.8 hours, 2.0 hours, 2.5
Hour, 2.8 hours), be again heated to 900-1000 DEG C of (such as 910 DEG C, 920 DEG C, 930 DEG C, 940 DEG C, 950 DEG C, 960 DEG C, 970
DEG C, 980 DEG C, 990 DEG C), keep the temperature 1-2 hours (such as 1.2 hours, 1.4 hours, 1.6 hours .8 hours, 1.9 hours), then plus
Heat to 1100-1200 DEG C (such as 1110 DEG C, 1120 DEG C, 1130 DEG C, 1140 DEG C, 1150 DEG C, 1160 DEG C, 1170 DEG C, 1180 DEG C,
1190 DEG C), heat preservation 2-4 hours (such as 2.2 hours, 2.5 hours, 2.8 hours, 3.1 hours, 3.4 hours, 3.7 hours, it is 3.9 small
When), it is again heated to 1300-1400 DEG C (such as 1320 DEG C, 1340 DEG C, 1360 DEG C, 1380 DEG C, 1390 DEG C), keeps the temperature 2-3 hours
(such as 2.2 hours, 2.4 hours, 2.6 hours, 2.8 hours), be again heated to 1500-1600 DEG C (such as 1520 DEG C, 1540 DEG C,
1560 DEG C, 1580 DEG C, 1590 DEG C), heat preservation 1-3 hours (such as 1.2 hours, 1.5 hours, 1.8 hours, 2.0 hours, it is 2.5 small
When, 2.8 hours), be again heated to 1700-1800 DEG C (such as 1720 DEG C, 1740 DEG C, 1760 DEG C, 1780 DEG C, 1790 DEG C), keep the temperature
It is 2-3 hours (such as 2.2 hours, 2.4 hours, 2.6 hours, 2.8 hours), finally heated to maximum sintering temperature 2000-2200
DEG C (such as 2030 DEG C, 2060 DEG C, 2090 DEG C, 2120 DEG C, 2150 DEG C, 2180 DEG C), heat preservation 3-5 hours (such as 3.3 hours, 3.6
Hour, 3.9 hours, 4.2 hours, 4.5 hours, 4.8 hours), high-density molybdenum slab is made, density reaches 10.0-10.15cm3/
g.The sintering slab obtained using preferred embodiment, interior tissue more dense uniform provide advantageous condition for rolling.
S4, rolling, rolls sintered slab in step S3, obtains rolled parts；The concrete operations side of the step
Method are as follows: split rolling method is carried out to sintered slab first, cogging temperature control is in 1150-1350 DEG C of (such as 1180 DEG C, 1210
DEG C, 1240 DEG C, 1270 DEG C, 1300 DEG C, 1330 DEG C), using melt down per pass cooling rolling by the way of, cool down 30-100 per pass
DEG C (such as 37 DEG C, 45 DEG C, 53 DEG C, 60 DEG C, 68 DEG C, 76 DEG C, 85 DEG C, 92 DEG C, 98 DEG C), final rolling temperature are not less than 700 DEG C,
Horizontal and vertical alternate tandem rolling mode is used during the rolling process, and drafts per pass is during the rolling process
The total deformation of 30%-40% (such as 32%, 34%, 36%, 38%, 39%), slab control the root between 90%-98%
Suitable total deformation is selected according to required plate thickness, obtains rolled parts；Then obtained rolled parts is subjected to final annealing process；?
Interspersed stress relief annealing process during tandem rolling, 700-850 DEG C of stress relief annealing temperature (such as 720 DEG C, 740 DEG C, 760
DEG C, 780 DEG C, 800 DEG C, 820 DEG C, 840 DEG C), to temperature heat preservation 0.5-1.5 hours (such as 0.6 hour, 0.8 hour, 1.0 hours,
1.2 hours, 1.4 hours), fire time deformation amount controlling 40%-80% (such as 45%, 50%, 55%, 60%, 65%, 70%,
75%)；Fire time deflection herein refers to the total deformation between the stress relief annealing of interval.The annealing temperature of final annealing process
For 850-920 DEG C (such as 860 DEG C, 870 DEG C, 880 DEG C, 890 DEG C, 900 DEG C, 910 DEG C), to temperature heat preservation, (1.1 is small within 1-1.5 hours
When, 1.2 hours, 1.3 hours, 1.4 hours).Mechanics Performance Testing, test annealing finally are carried out to the rolled parts after final annealing
The fracture elongation of treated rolled parts, it is desirable that reach 20%-30%.Stress relief annealing can be eliminated in the operation of rolling in time and be produced
Raw internal stress, but must assure that and do not recrystallized in annealing process, so the temperature control and heat preservation of stress relief annealing
Time control is extremely important.Rolled parts interior tissue after final annealing process is that tiny fibr tissue and being mingled with some is tied again
Crystalline substance tissue, tiny fibr tissue are mingled with the rotary pressure deformation that recrystallized structure is more advantageous to the later period, are more conducive to process big major diameter
The crucible product of ratio.
S5, surface treatment, is surface-treated rolled parts obtained in step S4, removes the surface defect of rolled parts,
(alkali cleaning, 400-650 DEG C of alkali liquid temperature, lye used can be the hydrogen of molten condition to the oxide skin on cleaning removal rolled parts surface
Sodium oxide molybdena, the purity 99wt% of sodium hydroxide), the local defects such as pit, the crackle on rolled parts surface are polished off, to obtain
The finished product of molybdenum plate rolled parts.
Heretofore described big L/D ratio molybdenum crucible is preferably the molybdenum crucible that draw ratio is 4-5.
Embodiment 1
The spinning molybdenum plate with a thickness of 4.8mm is prepared, is specifically comprised the following steps:
S1 feeds intake, and chooses the mold such as gum cover mould with a thickness of 60mm, is packed into molybdenum powder.
S2, die mould carry out die mould to the mold equipped with powder chosen in step S1 using the forming method of isostatic cool pressing；
The pressure that die mould uses is 220MPa, and pressure maintaining 20 minutes.After die mould processing, to the slab after die mould according in sintering process
Shrinkage ratio carries out shaping, to guarantee that sintered slab is smooth intact.
S3, sintering, is sintered the slab after step S2 medium-pressure type；Slab after shaping is placed in intermediate frequency furnace and is carried out
Molybdenum plate blank is heated to 600 DEG C, keeps the temperature 1 hour, be again heated to 900 DEG C, keep the temperature 2 hours, be again heated to 1200 DEG C, protected by sintering
Temperature 4 hours is again heated to 1300 DEG C, keeps the temperature 2 hours, is again heated to 1600 DEG C, keeps the temperature 3 hours, is again heated to 1700 DEG C, heat preservation
3 hours, finally heated to 2000 DEG C, 5 hours are kept the temperature, high-density molybdenum slab is made, density reaches 10.05cm3/g。
S4, rolling carry out split rolling method to sintered slab first, and cogging temperature is controlled at 1150 DEG C, using per pass
The secondary mode for melting down cooling rolling, 30 DEG C of cooling every time, final rolling temperature is not less than 700 DEG C, during the rolling process using cross
To with longitudinal alternate tandem rolling mode, drafts per pass is 35% during the rolling process, and the total deformation of slab is
92%.Intert 1 stress relief annealing during entire tandem rolling, annealing temperature is set as 830 DEG C, keeps the temperature 0.5 hour, rolls
Obtained after system rolled parts with a thickness of 4.8mm, the molybdenum plate of the thickness can be spun to the crucible that wall thickness is 3mm, and the molybdenum of this thickness
Board finished product rate is higher, can reach 95% or more；Then by obtained rolled parts carry out final annealing process, 900 DEG C of annealing temperature,
Heat preservation 1 hour；Molybdenum plate mechanical property after final annealing process is preferable, and fracture elongation can control 25% or more；Most
Rolled parts after choosing final annealing afterwards carries out Mechanics Performance Testing, the fracture elongation of the rolled parts after measuring annealing,
The fracture elongation of rolled parts longitudinal direction reaches 27%, and the fracture elongation of rolled parts transverse direction reaches 25.5%.Using optical microphotograph
Mirror carries out observation shooting to molybdenum plate made from the rolling mill practice, obtains metallurgical tissue picture such as Fig. 4.
S5, surface treatment, is surface-treated rolled parts obtained in step S4, removes the surface defect of rolled parts,
The oxide skin (alkali cleaning, 600 DEG C of alkali liquid temperature) on cleaning removal rolled parts surface, polishes off pit, the crackle on rolled parts surface
Etc. local defects, to obtain the finished product of molybdenum plate rolled parts.
S6, blanking, water knife are cut into the blank of Φ 150*4.8mm size.
S7, selects suitable spinning moulds of industrial equipment, molybdenum plate is heated to 600-800 DEG C using flame gun, in spinning
Rotary pressure deformation is carried out on machine, this spinning temperature is determined by the institutional framework of molybdenum plate, is had fiber fines tissue and is mingled with one
The tissue for the recrystallization divided is easier to deform at this temperature, according to the corresponding spinning road of the dimensioned of big L/D ratio molybdenum crucible
Diameter.
S8, machining vehicle cut shape, and cleaning polishing crucible surface is to get finished product crucible.Its final size is general are as follows: crucible
Height about 170mm, base diameter 36mm, crucible opening diameter 48mm, crucible bottom thickness 4.8mm, crucible wall thickness 3mm, this
The defects of crucible is used above at 1800 DEG C, and the service life can reach 350 hours or more, and crackle and obvious deformation are found no after use
It generates.
Embodiment 2
The spinning molybdenum plate with a thickness of 2.5mm is prepared, is specifically comprised the following steps:
S1 feeds intake, and chooses the mold such as gum cover mould with a thickness of 50mm, is packed into molybdenum powder.
S2, die mould carry out die mould to the mold equipped with powder chosen in step S1 using the forming method of isostatic cool pressing；
The pressure that die mould uses is 200MPa, and pressure maintaining 30 minutes.After die mould processing, to the slab after die mould according in sintering process
Shrinkage ratio carries out shaping, to guarantee that sintered slab is smooth intact.
Molybdenum plate blank is heated to 700 DEG C, keeps the temperature 2 hours, be again heated to 1000 DEG C, keep the temperature 2 hours, reheated by S3, sintering
To 1200 DEG C, 2 hours are kept the temperature, is again heated to 1400 DEG C, keeps the temperature 3 hours, is again heated to 1500 DEG C, 3 hours is kept the temperature, is again heated to
1800 DEG C, 2 hours are kept the temperature, finally heated to 2100 DEG C, 5 hours is kept the temperature, high-density molybdenum slab is made, density reaches
10.12cm3/g。
S4, rolling carry out split rolling method to sintered slab first, and cogging temperature is controlled at 1200 DEG C, using per pass
The secondary mode for melting down cooling rolling, 50 DEG C of cooling every time, final rolling temperature is not less than 700 DEG C, during the rolling process using cross
To with longitudinal alternate tandem rolling mode, drafts per pass is 30% during the rolling process, and the total deformation of slab is
95%, 1 stress relief annealing is interted during tandem rolling, annealing temperature is set as 800 DEG C, keeps the temperature 1 hour, obtains after rolling
Rolled parts with a thickness of 2.5mm, the molybdenum plate of the thickness can be spun to the crucible that wall thickness is 1.5mm, and the molybdenum plate finished product of this thickness
Rate is higher, can reach 92% or more, and obtained rolled parts is then carried out final annealing process, 850 DEG C of annealing temperature, keeps the temperature 1
Hour；Molybdenum plate mechanical property after final annealing process is preferable, and fracture elongation can control 20% or more；It finally chooses most
The rolled parts after annealing carries out Mechanics Performance Testing, the fracture elongation of the rolled parts after measurement annealing, rolling eventually
The fracture elongation of part longitudinal direction reaches 25%, and the fracture elongation of rolled parts transverse direction reaches 22%.
S5, surface treatment, is surface-treated rolled parts obtained in step S4, removes the surface defect of rolled parts,
The oxide skin (alkali cleaning, 600 DEG C of alkali liquid temperature) on cleaning removal rolled parts surface, polishes off pit, the crackle on rolled parts surface
Etc. local defects, to obtain the finished product of molybdenum plate rolled parts.
S6, blanking, water knife are cut into the blank of Φ 160*2.5mm size.
S7 selects suitable spinning moulds of industrial equipment, by heating of plate blank to the 700-800 DEG C of progress spinning change on spinning machine
Shape, spinning temperature are determined have fiber fines tissue and be mingled with the tissue of the recrystallization of a part by the institutional framework of molybdenum plate
It is easier to deform at this temperature, according to the corresponding spinning path of the dimensioned of big L/D ratio molybdenum crucible.
S8, machining vehicle cut shape, and cleaning polishing crucible surface is to get finished product crucible.Its final size is general are as follows: crucible
Height about 165mm, base diameter 34mm, crucible opening diameter 48mm, crucible bottom thickness 2.5mm, crucible wall thickness 1.5mm.
This crucible is used above at 2000 DEG C, and the service life can reach 200 hours or more, and crackle and obvious deformation etc. are found no after use and is lacked
It falls into and generates.
Embodiment 3
The present embodiment is in addition to sintering process is different from embodiment 1, other processing steps are the same as embodiment 1.The embodiment
Sintering process is to be warming up to 2000 DEG C with the speed of 10 DEG C/min, and keep the temperature 5h, and obtained molybdenum plate blank density is 9.6cm3/g。
Fracture elongation using the rolled parts longitudinal direction obtained after the rolling mill practice rolling of embodiment 1 reaches 15%, rolling
The fracture elongation of part transverse direction reaches 10%.
Embodiment 4
The present embodiment is in addition to rolling mill practice is different from embodiment 1, other processing steps are the same as embodiment 1.The present embodiment
Rolling mill practice is as follows: split rolling method carried out to sintered slab first, 1350 DEG C of cogging temperature, and using melting down cooling per pass
The mode of rolling, every time 100 DEG C of cooling, final rolling temperature are not less than 700 DEG C, use horizontal and vertical friendship during the rolling process
The tandem rolling mode replaced, drafts per pass is 35% during the rolling process, and the total deformation of slab is 92%.Entire
Intert 1 stress relief annealing during tandem rolling, annealing temperature is set as 800 DEG C, keeps the temperature 1 hour, is rolled after rolling
Part with a thickness of 4.8mm, the molybdenum plate of the thickness can be spun to the crucible that wall thickness is 3mm, and the molybdenum plate yield rate of this thickness is higher,
90% or more can be reached；Then obtained rolled parts is subjected to final annealing process, 880 DEG C of annealing temperature, keeps the temperature 1 hour；Through
Molybdenum plate mechanical property after crossing final annealing process is preferable, and fracture elongation can control 20% or more；It finally chooses and finally moves back
Fire treated rolled parts carries out Mechanics Performance Testing, the fracture elongation of the rolled parts after measurement annealing, and rolled parts is vertical
To fracture elongation reach 22%, the fracture elongation of rolled parts transverse direction reaches 20%.
Comparative example 1
This comparative example carries out molybdenum plate rolling using common rolling mill practice, this comparative example is different from embodiment 1 except rolling mill practice,
Other processing steps are the same as embodiment 1.The rolling mill practice of this comparative example is as follows: split rolling method is carried out to sintered slab first,
Cogging temperature is controlled at 1100-1300 DEG C, by the way of melting down cooling rolling per pass, is cooled down 50-100 DEG C per pass, most
Whole rolling temperature is not less than 750 DEG C, and drafts per pass is 15-20% during the rolling process, and the total deformation of slab controls
Between 80-90%, suitable total deformation is selected according to required plate thickness, obtains rolled parts；Then by obtained rolled parts into
Row final annealing process, interts stress relief annealing process during the rolling process, and 750-850 DEG C of stress relief annealing temperature keeps the temperature 1-
1.5 hours, fire time deformation amount controlling was in 40%-80%；The annealing temperature of final annealing process is 950-1050 DEG C, keeps the temperature 1-
1.5 hour.Mechanics Performance Testing finally is carried out to the rolled parts after final annealing, the fracture of rolled parts is prolonged after test annealing
Rate is stretched, fracture elongation 15% carries out observation bat using tissue of the optical microscopy to molybdenum plate made from the rolling mill practice
It takes the photograph, obtains metallurgical tissue picture such as Fig. 3.
The metallurgical tissue picture of comparison diagram 3 and Fig. 4 can be seen that under same amplification factor (200x), according to this hair
The molybdenum plate that bright embodiment 1 rolls out, obtains thinner fibr tissue, and is mingled with including some recrystallized structures, and such group
It knits and is easier to rotary pressure deformation, and the molybdenum plate that common process rolls out in comparative example 1, metallographic are shown, fibr tissue is thicker, and does not have
Including having recrystallized structure, such group is woven in spinning process the phenomenon that being easy to appear spinning tearing, so as to cause product report
It is useless.
In conclusion a kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate provided by the invention, by cold etc.
Static pressure technology carries out die mould to powder, obtains the slab of higher density, is sintered by sintering method to the slab after die mould,
To improve its total quality；The rolling of aximal deformation value is carried out to sintered slab by the method for tandem rolling, it is available
Isotropic fiber fines shape tissue, and vertically and horizontally tissue mutually overlap joint interlocks, tissue arrangement is uniform sequential, can effectively keep away
Exempt from it is each to discontinuity when the defect that generates, provide advantageous condition for subsequent spinning, the present invention is using isostatic cool pressing, sintering
Molybdenum raw material slab is processed with the tandem rolling method of aximal deformation value, the spinning for making it meet big L/D ratio molybdenum crucible is wanted
It asks, has great importance to the production of big L/D ratio molybdenum crucible.
The above description is only a preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate, which is characterized in that the milling method includes as follows
Step:
S1 feeds intake, and according to required molybdenum plate blank size, chooses the mold of suitable dimension, carries out dress powder；
S2, die mould carry out die mould processing to the mold for filling powder in step S1, the slab of suitable thickness are made；
S3, sintering are sintered the slab obtained of pressure in step S2；
S4, rolling, rolls sintered slab in step S3, obtains rolled parts；
S5, surface treatment, is surface-treated rolled parts obtained in step S4, removes the surface defect of the rolled parts,
Obtain molybdenum plate rolled parts finished product.
2. a kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as described in claim 1, which is characterized in that described
In step S2, using etc. static pressure forming method in step S1 fill powder mold carry out die mould.
3. a kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as described in claim 1, which is characterized in that described
In step S2, die mould is carried out to the slab chosen in step S1 using the forming method of isostatic cool pressing, the pressure that die mould uses for
200-220MPa, pressure maintaining 10-30 minutes.
4. a kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as described in claim 1, which is characterized in that also wrap
Shaping is included, shaping is carried out according to the shrinkage ratio in sintering process to slab obtained in step S2, to guarantee to obtain institute after being sintered
Need size, smooth intact slab.
5. a kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as claimed in claim 4, which is characterized in that described
In step S3, the slab after shaping is placed in sintering furnace and is sintered, maximum sintering temperature is 2000-2200 DEG C, keeps the temperature 3-5
Hour.
6. a kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as claimed in claim 5, which is characterized in that described
Sintering furnace uses intermediate frequency furnace.
7. a kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as described in claim 1, which is characterized in that described
Step S4 concrete operation method are as follows: tandem rolling is carried out to slab sintered in the step S3 first, obtains rolled parts；So
Obtained rolled parts is subjected to final annealing process afterwards；Rolled parts after finally extracting final annealing process carries out mechanical property survey
Examination, the fracture elongation of rolled parts after test annealing.
8. a kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as claimed in claim 7, which is characterized in that described
During tandem rolling, split rolling method is carried out to slab sintered in step S3 first, cogging temperature is controlled in 1150-1350
DEG C, by the way of melting down cooling rolling per pass, cooling down 30-100 DEG C per pass, final rolling temperature is not less than 700 DEG C,
Horizontal and vertical alternate tandem rolling mode is used in the operation of rolling, tandem rolling obtains rolled parts；
Preferably, drafts during the rolling process per pass is 30%-40%；
More preferably, the total deformation of slab is controlled between 90%-98%.
9. a kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as described in claim 1, which is characterized in that described
The concrete operations of step S5 are as follows: cleaning polishing is carried out to the surface of rolled parts obtained in step S4, removes the rolled parts table
The oxide skin in face polishes off pit, the crackle local defect on the rolled parts surface.
10. a kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate as claimed in claim 7, which is characterized in that institute
State tandem rolling interspersed stress relief annealing process in the process, 700-850 DEG C of the temperature of the stress relief annealing；The final annealing
The annealing temperature of processing is 850-920 DEG C.
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Effective date of registration: 20211228 Address after: 301800 Baozhong Road 10, energy conservation and environmental protection industrial zone, Baodi District, Tianjin Patentee after: ATTL ADVANCED MATERIALS Co.,Ltd. Patentee after: Advanced Technology & Materials co., ltd Address before: 101117 in Zhaoli Industrial Zone, Hugezhuang, Lucheng Town, Tongzhou District, Beijing Patentee before: ATTL ADVANCED MATERIALS Co.,Ltd. Patentee before: ATTL (TIANJIN) ADVANCED TECHNOLOGY & MATERIALS Co.,Ltd. Patentee before: ADVANCED TECHNOLOGY & MATERIALS Co.,Ltd. |